CN110835262A - Blue-green hard luminous stone with zirconium-niobium ion common luminous center and preparation method thereof - Google Patents
Blue-green hard luminous stone with zirconium-niobium ion common luminous center and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a blue-green hard luminous stone with a zirconium-niobium ion co-luminous center and a preparation method thereof, wherein the blue-green hard luminous stone is prepared from xNd zirconium-niobium ion co-luminous center blue-green luminous powder serving as a main material2O3·(1‑1.5x)ZrO2·(1‑0.6y)P2O5·yAl2O3(x = 0.002-0.08; y = 0.001-0.15) and a mixture of magnesium aluminate powder as an auxiliary material, and the mixture is subjected to mixing and tabletting and then is subjected to high-temperature calcination in a reducing atmosphere to obtain the magnesium aluminate tablet. The hard luminous stone prepared by the invention can emit bright blue-green light after being irradiated by lamplight, can continuously emit light for more than 13 hours in the dark after the illumination is stopped, has high hardness, has Mohs hardness of 6.3-7.5 Mohs as tested by a jade hardness tester, has glittering and translucent surface after being polished and polished, and has good ornamental valueAnd (4) value.
Description
Technical Field
The invention belongs to the field of luminescent material preparation, and particularly relates to a zirconium-niobium ion co-luminescent center blue-green hard luminescent stone and a preparation method thereof.
Background
The long afterglow luminescent material is also called light storage type self luminescent material, can absorb sunlight, ultraviolet light, stray light and the like to store energy, generates afterglow effect after stopping the excitation of the light source, and continuously emits light. Hitherto, long-afterglow luminescent material products have the characteristics of luminescent coatings, luminescent ceramics, luminescent rubber, luminescent leather, luminescent glass, luminescent decorative stone and the like, have good chemical stability, photoluminescence, energy conservation, environmental protection and the like, and are called as decorative luminescent materials with development prospects in the 21 st century. The long-afterglow luminescent material consists of a main material and an activator (and an auxiliary activator). The long-afterglow luminescent materials reported at present mainly comprise different host materials which are doped with activators and serve as luminescent centers of the materials, so that the luminescent performance of the host materials is improved. Such as the invention patent' a Mn2+The doped yellow long afterglow luminescent material and its preparation method (application number: 201710651844.6) disclose a Mn2+The chemical expression of the doped yellow long afterglow luminescent material is Ca2-xSn2-yAl2O9:xMn2+,yR3+(ii) a Wherein x is more than or equal to 0.002 and less than or equal to 0.080 and 0<y is less than or equal to 0.120; r = Tb, Ce, Dy, Tm, Nd, Gd, Y, Er, La, Pr, Sm, Yb, Lu or Ho, wherein Ca2Sn2Al2O9As a host material, Mn2+Is an activator, and the R ion is an auxiliary activator.
In nature, many ores have long-afterglow luminescent characteristics, and the materials are used for manufacturing various articles such as luminous cups, luminous pearls and the like due to the special luminescent characteristics of the materials. The light-storing self-luminous material is used for imitating natural luminous pearl to manufacture luminous stone, so that the expensive manufacturing cost of ore can be reduced, and the material tends to be commercialized. The invention provides a zirconium-niobium ion co-luminescence center blue-green hard luminescent stone, which has good luminescence performance and commercial application prospect.
Disclosure of Invention
The invention aims to provide a blue-green hard luminous stone with a zirconium-niobium ion co-luminescence center and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a blue-green hard luminescent stone with Zr-Nb ion common luminescent center is prepared from main material of blue-green luminescent powder xNd with Zr-Nb ion common luminescent center2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3(x = 0.002-0.08; y = 0.001-0.15) and a mixture of magnesium aluminate powder as an auxiliary material, and then the mixture is subjected to mixing and tabletting and is calcined at high temperature in a reducing atmosphere. The introduction of the magnesium aluminate powder as an auxiliary material plays a great role in the hardness of the luminolite. The weight percentage of the double-luminescence center blue-green luminescent powder is 85-95%, the weight percentage of the magnesium aluminate powder is 5-15%, and the sum of the weight percentages of the two is 100%.
The preparation method of the blue-green hard luminescent stone with the zirconium-niobium ion co-luminescence center comprises the steps of mixing a mixture of blue-green luminescent powder with the zirconium-niobium ion co-luminescence center and magnesium aluminate powder which are respectively weighed, adding deionized water for wetting, curing for 2-3 hours in a closed container, tabletting and forming by a tablet press under the pressure of 6-26 atmospheric pressures, placing in a reducing atmosphere, and calcining for 2-5 hours at 950-1200 ℃ to obtain the blue-green hard luminescent stone.
Further, the reducing atmosphere is composed of H2And N2Mixed gas or CO gas which is formed by 2-5: 98-95 volume ratio.
The zirconium-niobium ion co-luminescence center blue-green luminescent powder is prepared into a sample in a weak reducing atmosphere by adopting a preparation process of high-temperature presintering, tabletting, high-temperature calcining and crushing; the preparation method comprises the following steps:
a blue-green luminescent powder with Zr-Nb ion common luminescent center has chemical composition of xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3(x=0.002~0.08; y= 0.001~0.15)。
The preparation method comprises the following steps:
1) respectively weighing raw material nano ZrO according to stoichiometric ratio2、NH4H2PO4、Nd2O3、Al2O3And press xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3Weighing fluxing agent H with the mol percentage of 2-20 mol% (x = 0.002-0.08; y = 0.001-0.15)3BO3；
2) Mixing the weighed raw materials, placing the mixture in a ball milling tank, adding absolute ethyl alcohol to the position of half of the height of the tank, grinding the mixture for 2 to 4 hours at the rotating speed of 600 to 1000 r/min, taking the raw material mixture out of a crucible, air-drying the mixture for half an hour at the temperature of 100 ℃, and transferring the mixture to the crucible;
3) placing a crucible in a box furnace, presintering for 2 hours at 900 ℃ to obtain product precursor powder, cooling, placing the product precursor powder in a ball milling tank, adding absolute ethyl alcohol to the position of half of the height of the tank, grinding for 2-4 hours at the rotating speed of 600-1000 r/min, taking the product precursor powder out of the ball milling tank, air drying for half an hour at 100 ℃, pressing into a sheet by a press machine at the pressure of 5-15 atmospheric pressures, placing the sheet in the crucible in a weak reducing atmosphere (H)2、N2Or CO) at 950-1200 ℃ for 3-4 hours to prepare the blue-green long-afterglow luminescent material block xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3(x = 0.002-0.08; y = 0.001-0.15). The luminescent material block is crushed by a crusher or ground by an agate mortar to form luminescent powder.
Has the advantages that: the hard luminous stone prepared by the invention can emit bright blue-green light after being irradiated by lamplight, can continuously emit light for more than 13 hours in the dark after the illumination is stopped, has high hardness, has Mohs hardness of 6.3-7.5 Mohs as tested by a jade hardness tester, has glittering and translucent surface after being polished and polished, and has good ornamental value.
Drawings
FIG. 1 is an XRD spectrum of a blue-green hard luminolite with a zirconium niobium ion co-luminescence center prepared by the invention;
FIG. 2 is an excitation emission spectrum of blue-green hard luminolite with zirconium-niobium ion co-luminescence center prepared by the invention.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
The best chemical composition of the blue-green luminescent powder with the zirconium-niobium ion common luminescent center in the technology is 0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3. The preparation method comprises the following steps:
1) respectively weighing raw material nano ZrO according to stoichiometric ratio2、NH4H2PO4、Nd2O3、Al2O3And according to 0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3The molar percentage of (A) is 8 mol%, and the fluxing agent H is weighed3BO3；
2) Mixing the weighed raw materials, placing the mixture in a ball milling tank, adding absolute ethyl alcohol to the position of half of the height of the tank, grinding the mixture for 3 hours at the rotating speed of 800r/min, taking out the raw material mixture, airing the mixture for half an hour at the temperature of 100 ℃, and transferring the mixture into a crucible;
3) placing a crucible in a box furnace, presintering for 2 hours at 900 ℃ to obtain product precursor powder, cooling, placing the product precursor powder in a ball milling tank, adding absolute ethyl alcohol to the position of half of the height of the tank, grinding for 3 hours at the rotating speed of 800r/min, taking the product precursor powder out of the ball milling tank, air-drying for half an hour at 100 ℃, pressing into a sheet by a press machine under the pressure of 12 atmospheres, placing the sheet in the crucible under a weak reducing atmosphere (H)2、N2Or CO) at 1200 deg.C for 3 hr to obtain blue-green long-afterglow luminescent material 0.006Nd2O3·0.991ZrO2·0.97P2O5·0.05Al2O3。
Example 1
Zirconium chelateNiobium ion common luminous center blue-green luminous powder (0.006 Nd)2O3·0.991ZrO2·0.97P2O5·0.05Al2O3) 85 percent of the zirconium niobium ion co-luminous center blue-green luminous powder (0.006 Nd) and 5 percent of the magnesium aluminate powder2O3·0.991ZrO2·0.97P2O5·0.05Al2O3) And magnesium aluminate powder are mixed, added with deionized water for wetting, cured in a closed container for 2 hours, then tabletted and molded by a tabletting machine under the pressure of 6 atmospheric pressures, and then placed in a CO reducing atmosphere for calcining at 950 ℃ for 2 hours to prepare the blue-green hard luminescent stone. The afterglow time of the prepared luminous stone is 9 hours, and the Mohs hardness is 5.0.
Example 2
Blue-green luminescent powder (0.006 Nd) with zirconium-niobium ion common luminescent center2O3·0.991ZrO2·0.97P2O5·0.05Al2O3) 90 percent of the zirconium niobium ion co-luminous center blue-green luminous powder (0.006 Nd) and 10 percent of the magnesium aluminate powder2O3·0.991ZrO2·0.97P2O5·0.05Al2O3) Mixing with magnesium aluminate powder, wetting with deionized water, aging in a sealed container for 2 hr, tabletting under 26 atm, and placing in H2/N2(H2And N25 percent by volume to 95 percent by volume) in reducing atmosphere, and calcining for 3 hours at 1150 ℃ to obtain the blue-green hard luminous stone. The afterglow time of the prepared luminous stone is 13 hours, and the Mohs hardness is 7.5.
Example 3
Blue-green luminescent powder (0.006 Nd) with zirconium-niobium ion common luminescent center2O3·0.991ZrO2·0.97P2O5·0.05Al2O3) The weight percentage of the zirconium niobium ions is 95 percent, the weight percentage of the magnesium aluminate powder is 5 percent, and the zirconium niobium ions which are respectively weighed jointly emit lightCenter blue-green luminescent powder (0.006 Nd)2O3·0.991ZrO2·0.97P2O5·0.05Al2O3) Mixing with magnesium aluminate powder, wetting with deionized water, aging in a sealed container for 3 hr, tabletting under 15 atmospheric pressure with a tabletting machine, and placing in H2/N2(H2And N2The volume ratio is 3 percent to 97 percent) and calcining for 5 hours at 1200 ℃ in reducing atmosphere to prepare the blue-green hard luminous stone. The afterglow time of the prepared luminous stone is 11 hours, and the Mohs hardness is 6.5.
FIG. 1 is an XRD spectrum of a blue-green hard luminolite with a zirconium niobium ion common luminescence center, wherein the phase of a sample prepared by the technology mainly comprises phase PDF #49-1079, phase PDF #21-1152 and part of phase PDF # 36-0352. FIG. 2 shows the excitation emission spectrum of blue-green hard luminolite with zirconium-niobium ion co-luminescence center, 487 nm belonging to the blue light range and 521 nm and 545 nm falling in the green light range.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (4)
1. The blue-green hard luminous stone with the zirconium-niobium ion common luminous center is characterized in that: the material is prepared by mixing, tabletting and calcining a zirconium niobium ion co-luminescent center blue-green luminescent powder serving as a main material and a magnesium aluminate powder mixture serving as an auxiliary material at a high temperature in a reducing atmosphere; the chemical composition of the zirconium-niobium ion co-luminescence center blue-green luminescent powder is xNd2O3·(1-1.5x)ZrO2·(1-0.6y)P2O5·yAl2O3；x=0.002~0.08；y= 0.001~0.15。
2. The hard zircon niobium ion co-luminescent center blue-green luminolite of claim 1, wherein: the weight percentage of the zirconium niobium ion common luminescence center blue-green luminescent powder in the zirconium niobium ion common luminescence center blue-green hard luminescent stone is 85-95%, the weight percentage of the magnesium aluminate powder is 5-15%, and the sum of the weight percentages of the two is 100%.
3. A method for preparing a hard blue-green luminolite having a zirconium niobium ion co-luminescence center as claimed in any one of claims 1-2, wherein: mixing the zirconium-niobium ion co-luminescence center blue-green luminescent powder and magnesium aluminate powder mixture, adding deionized water for wetting, curing for 2-3 hours in a closed container, then tabletting and forming by a tabletting machine under the pressure of 6-26 atmospheric pressures, placing in a reducing atmosphere, and calcining for 2-5 hours at 950-1200 ℃ to obtain the zirconium-niobium ion co-luminescence center blue-green luminescent stone.
4. The production method according to claim 3, characterized in that: the reducing atmosphere is composed of H2And N2Mixed gas or CO gas which is formed by 2-5: 98-95 volume ratio.
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